CN1159414C - Zirconium containing asphalt and preparation method thereof - Google Patents
Zirconium containing asphalt and preparation method thereof Download PDFInfo
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- CN1159414C CN1159414C CNB011160233A CN01116023A CN1159414C CN 1159414 C CN1159414 C CN 1159414C CN B011160233 A CNB011160233 A CN B011160233A CN 01116023 A CN01116023 A CN 01116023A CN 1159414 C CN1159414 C CN 1159414C
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- zirconium
- containing asphalt
- pitch
- asphalt
- zirconium containing
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Abstract
The present invention discloses a zirconium-containing asphalt and a preparation method thereof. The asphalt has a softening point of 85 to 140 DEG C (ring and ball method GB2294-80) and contains 50 to 70 wt% of carbonized residue (carbon production rate GB-8729-89) and 1 to 10 wt% of zirconium. The preparation method comprises: primarily filtering or distilling coal tar or asphalt to remove once quinoline insoluble substances, then adding zirconium chloride according to the weight ratio of coal tar or asphalt: zirconium chloride =100: 1 to 20 in an anhyrous anaerobic atmosphere, increasing pressure at 280 to 420 DEG C or at 0.3 to 1.0MPa, reacting for 4 to 10 hrs so as to obtain the zirconium-containing asphalt. The zirconium-containing asphalt with good physical and chemical stability is a superior impregnant raw material and can also be used as an adhesive.
Description
The present invention relates to a kind of Zirconium containing asphalt and preparation method thereof.
Charcoal and graphite material have good intensity and modulus, and its high-temperature mechanical property is also very superior, therefore, except structure, friction and field of functional materials are applied, also is commonly used under the hot conditions.But oxidation and ablation can take place in pure charcoal and graphite material in high temperature oxidation atmosphere, the U.S. points out in 76-609 number AIAA in 1976 " solid booster rocket engine jet pipe with charcoal raw material of wood-charcoal material " report, add element formation refractory carbides such as zirconium, can improve the anti-oxidant and anti-ablation property of material.
Pitch is the basic raw material of making the raw material of wood-charcoal material, and it is to enter in the carbon matrix in related process as binding agent or soaker, if pitch carries zr element, just can make zirconic raw material of wood-charcoal material, improves the anti-oxidant and anti-ablative of raw material of wood-charcoal material.At present the anti-ablation raw material of wood-charcoal material of making zirconium carbide often adopts the adulterated method of micro mist, by with zirconic compound, as ZrO
2, the trifling level of ZrC powder is dispersed in the asphalt stock it by the certain physical means, zirconium enters in the material with pitch and becomes the raw material of wood-charcoal material that contains zirconium carbide in the pyrographite stage.
Mixing with micro mist different is, the present invention adopts the method for chemical reaction, makes zr element and asphaltene molecule formation compound, is Chemical bond between the two, and the distribution of zr element is more even in the pitch that obtains like this.
By inscription on pottery field, Li Xinyi chief editor, Chemical Industry Press published " modern chemistry reagent handbook in 1992, the 5th fascicle organometallic reagent " introduced common zirconium organic compound in the 584-592 page or leaf in air, in the water or chemical reaction, poor stability easily take place in the daylight.
The purpose of this invention is to provide a kind of in air, Zirconium containing asphalt of good stability and preparation method thereof in the water or in the daylight.
Zirconium containing asphalt softening temperature of the present invention is 85～140 ℃ (ring and ball method GB2294-80), and charred residue (producing carbon rate GB-8729-89) weight percent is 50～70%, and weight percent zirconia content is 1～10%.
Preparation method's concrete steps of Zirconium containing asphalt of the present invention are as follows: coal tar or pitch were filtered through the initial stage or not fusant of quinoline is removed in distillation, then in anhydrous, oxygen-free atmosphere, zirconium is pressed following weight ratio: coal tar or pitch: zirconium chloride=100: 1～20 add zirconium chlorides, under 280～420 ℃, from boosting or under 0.3～1.0Mpa, reacting, reacted 4～10 hours, and can obtain Zirconium containing asphalt.
Above-mentioned pitch can be coal-tar pitch or petroleum pitch.
Above-mentioned zirconium chloride can be tri-chlorination zirconium or zirconium tetrachloride, preferably zirconium tetrachloride.
Preferably 330～380 ℃ of above-mentioned temperature of reaction.
Zirconium containing asphalt of the present invention is compared with existing pitch has following advantage:
1. Zirconium containing asphalt physics of the present invention and chemical stability are good, and be slow 320 ℃ of following thermal responses, and can keeping for a long time in empty G﹠W, character does not change.
2. the MV minium viscosity of Zirconium containing asphalt of the present invention in the scope in 200～350 ℃ of intervals is good soaker raw material between 0.01～0.1Pa.s, also can be used as binding agent and uses.
3. the distribution of zr element is more even than the distribution of physical doping method in the Zirconium containing asphalt of the present invention.
Embodiments of the invention are as follows:
Embodiment 1
Get coal-tar pitch 200 grams of 68 ℃ of no quinoline insolubleses of softening temperature, zirconium tetrachloride 5 grams reacted 5 hours down from boosting at 350 ℃, obtained Zirconium containing asphalt, and softening temperature is 105 ℃, contains zirconium 1.64wt%, produces the pitch of carbon rate 62.5wt%.
Embodiment 2
Get coal-tar pitch 200 gram of 68 ℃ of no quinoline insolubleses of softening temperature, zirconium tetrachloride 5 grams, reaction is 10 hours under 280 ℃, 0.1Mpa pressure, obtains Zirconium containing asphalt, and softening temperature is 85 ℃, contains zirconium 1.46wt%, produces the pitch of carbon rate 50.5wt%.
Embodiment 3
Get coal-tar pitch 200 grams of 68 ℃ of no quinoline insolubleses of softening temperature, zirconium tetrachloride 5 grams reacted 5 hours down from boosting at 420 ℃, obtained Zirconium containing asphalt, and softening temperature is 138 ℃, contains zirconium 1.87wt%, produces the pitch of carbon rate 69.5wt%.
Embodiment 4
Get coal-tar pitch 200 grams of 68 ℃ of no quinoline insolubleses of softening temperature, zirconium tetrachloride 15 grams reacted 4 hours down from boosting at 350 ℃, obtained Zirconium containing asphalt, and softening temperature is 115 ℃, contains zirconium 5.01wt%, produces the pitch of carbon rate 64.5wt%.
Embodiment 5
Get coal-tar pitch 200 grams of 68 ℃ of no quinoline insolubleses of softening temperature, zirconium tetrachloride 40 grams reacted 5 hours down from boosting at 350 ℃, obtained Zirconium containing asphalt, and softening temperature is 137 ℃, contains zirconium 9.01wt%, produces the pitch of carbon rate 69.5wt%.
Embodiment 6
Get coal-tar pitch 200 grams of 68 ℃ of no quinoline insolubleses of softening temperature, tri-chlorination zirconium 5 grams reacted 5 hours down from boosting at 350 ℃, obtained Zirconium containing asphalt, and softening temperature is 98 ℃, contains zirconium 1.78wt%, produces the pitch of carbon rate 57.2wt%.
Embodiment 7
Get coal tar 200 grams of liquid state, no quinoline insolubles, zirconium tetrachloride 10 grams reacted 10 hours down from boosting at 350 ℃, obtained Zirconium containing asphalt, and softening temperature is 93 ℃, contains zirconium 7.21wt%, produces the pitch of carbon rate 56.7wt%.
Embodiment 8
Get petroleum pitch 200 grams of 72 ℃ of no quinoline insolubleses of softening temperature, zirconium tetrachloride 5 grams reacted 5 hours down from boosting at 350 ℃, obtained Zirconium containing asphalt, and softening temperature is 95 ℃, contains zirconium 1.84wt%, produces the pitch of carbon rate 50.7wt%.
Claims (5)
1. a Zirconium containing asphalt is characterized in that softening temperature is 85～140 ℃, and the charred residue weight percent is 50～70%, and weight percent zirconia content is 1～10%.
2. method for preparing the described Zirconium containing asphalt of claim 1, it is characterized in that concrete steps are as follows: coal tar or pitch were filtered through the initial stage or not fusant of quinoline is removed in distillation, then in anhydrous, oxygen-free atmosphere, press following weight ratio: coal tar or pitch: zirconium chloride=100: 1～20 add zirconium chlorides, under 280～420 ℃, from boosting or under 0.3～1.0Mpa, reacting 4～10 hours, can obtain Zirconium containing asphalt.
3. a kind of method for preparing the described Zirconium containing asphalt of claim 1 as claimed in claim 2 is characterized in that described pitch is coal-tar pitch or petroleum pitch.
4. a kind of method for preparing the described Zirconium containing asphalt of claim 1 as claimed in claim 2 is characterized in that described zirconium chloride is tri-chlorination zirconium or zirconium tetrachloride.
5. a kind of method for preparing the described Zirconium containing asphalt of claim 1 as claimed in claim 2 is characterized in that this reaction carries out under 330～380 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011160233A CN1159414C (en) | 2001-05-10 | 2001-05-10 | Zirconium containing asphalt and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011160233A CN1159414C (en) | 2001-05-10 | 2001-05-10 | Zirconium containing asphalt and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1385494A CN1385494A (en) | 2002-12-18 |
| CN1159414C true CN1159414C (en) | 2004-07-28 |
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ID=4662341
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011160233A Expired - Fee Related CN1159414C (en) | 2001-05-10 | 2001-05-10 | Zirconium containing asphalt and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1159414C (en) |
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2001
- 2001-05-10 CN CNB011160233A patent/CN1159414C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1385494A (en) | 2002-12-18 |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20040728 Termination date: 20160510 |
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| CF01 | Termination of patent right due to non-payment of annual fee |